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CN110724460A - Preparation method of cerium-aluminum composite oxide polishing powder - Google Patents

Preparation method of cerium-aluminum composite oxide polishing powder Download PDF

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Publication number
CN110724460A
CN110724460A CN201911105224.8A CN201911105224A CN110724460A CN 110724460 A CN110724460 A CN 110724460A CN 201911105224 A CN201911105224 A CN 201911105224A CN 110724460 A CN110724460 A CN 110724460A
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cerium
solution
composite oxide
aluminum
polishing powder
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CN201911105224.8A
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刘通
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a preparation method of cerium-aluminum composite oxide polishing powder, and relates to the technical field of preparation of polishing materials. The composition of which is x Al2O3‑y CeO2The performance test result shows that the cerium-aluminum composite oxide polishing powder prepared by the invention has the advantages of fine and uniform particle size, good suspension property, high polishing speed, less scratch, good wear resistance and obvious synergistic polishing effect on substrates such as precision optical glass, liquid crystal panels, quartz glass, glass hard disks and the like, and has simple preparation process, cheap and easily obtained raw materials compared with the prior art, thereby being suitable for industrial production.

Description

Preparation method of cerium-aluminum composite oxide polishing powder
The technical field is as follows:
the invention relates to the technical field of preparation of polishing materials, in particular to a preparation method of cerium-aluminum composite oxide polishing powder.
Background art:
the combination and surface modification of polishing particles are important ways and means for improving the polishing efficiency and precision of polishing powder at present. Because the particle performance can be coordinated through the multi-element composition, and the dispersion stability, the polishing efficiency and the precision of the slurry can be improved through the ion surface modification. Alpha-alumina particles are widely used CMP abrasive materials at present, but the following problems exist in practical use: on one hand, the alpha-alumina abrasive particles have high hardness, and the surface is seriously damaged in the polishing process, so that the surface roughness is high, and surface defects such as polishing scratches, pits and the like are easy to occur; on the other hand, the dispersion stability of the particles is not good, the particles are easily agglomerated to form large particles, and the presence of the large particles is considered to be one of the sources of the generation of the polishing scratches.
In order to solve the problems, the surface of the alpha-alumina particle is modified by the cerium oxide with higher chemical activity, so that the dispersion stability of the particle is improved, the hardness of the alpha-alumina particle is properly reduced, and the alpha-alumina particle can be better applied to the field of high-grade optical processing.
The invention content is as follows:
in view of the disadvantages of the prior art, it is an object of the present invention to provide a method for producing a polishing material. The polishing material produced by the method can be suitable for the field of high-grade optical instrument processing, and particularly can be used for polishing precision optical glass.
In order to solve the technical problems, the invention adopts the technical scheme that the preparation method of the cerium-aluminum composite oxide polishing powder comprises the following steps:
A. preparing a colloidal solution:
(1) dispersing pseudo-boehmite into a certain amount of pure water under the condition of high-speed stirring to ensure that the mass percentage of the pseudo-boehmite is 10-20 percent, thus obtaining solid-liquid mixed slurry;
(2) slowly dripping concentrated inorganic acid solution into the solid-liquid mixed slurry for peptizing under the condition of keeping the stirring speed unchanged according to the acid/aluminum mass ratio of 0.1-0.45 to obtain aluminum hydroxide colloidal solution. The concentrated inorganic acid is hydrochloric acid and nitric acid, preferably hydrochloric acid;
(3) and adding a structure directing agent accounting for 1-3% of the total mass of the powder (pseudo-boehmite and cerium carbonate) into the aluminum hydroxide colloidal solution, and uniformly mixing to obtain a colloidal solution A. The structure directing agent is organic ammonium salt such as ammonium oxalate, ammonium succinate, ammonium tartrate, ammonium citrate, hexadecyl trimethyl ammonium bromide and the like, and preferably ammonium citrate; (ii) a
B. Preparing a mixed system:
(1) dissolving cerium carbonate in 38 wt% concentrated hydrochloric acid, controlling the pH value of the solution to be 1.3-1.8, and completely dissolving to obtain a clear cerium chloride solution;
(2) and filtering the cerium chloride solution, and then mixing the filtrate with aluminum: slowly adding cerium (0.1-0.5) in percentage by mass into the colloidal solution A to obtain a mixed system B;
C. coprecipitation:
(1) preparing sodium carbonate or ammonium bicarbonate into 1mol/L solution;
(2) adding 1mol/L sodium carbonate or ammonium bicarbonate solution into the mixed system B, performing precipitation reaction, controlling the pH value of the solution to be 6.5-7, and after the reaction is finished, performing vacuum filtration and deionized water leaching for three times to obtain a mixed precipitate C;
D. roasting and post-treatment:
(1) placing the mixed precipitate C in a muffle furnace, roasting at 750-950 ℃, keeping the temperature for 4-8 hours, and naturally cooling to obtain a polishing powder precursor;
(2) and crushing the polishing powder precursor to ensure that D50 is between 0.6 and 1.2 mu m and D90 is less than 3 mu m, thus obtaining the cerium-aluminum composite oxide polishing powder.
The preparation method of the cerium-aluminum composite oxide polishing powder takes the pseudo-boehmite and the cerium carbonate as raw materials, takes a small amount of structure directing agent as a composite medium, and adopts a coprecipitation method to prepare the cerium-aluminum composite oxide polishing powder. Compared with the prior art of the same type, the preparation process is relatively simple, the raw materials are low in price and wide in source, the method is suitable for industrial production, and the reaction process basically has no industrial three wastes, so that the method has the advantages of environmental friendliness, low energy consumption, high benefit and the like. Meanwhile, the prepared cerium-aluminum composite oxide polishing powder is fine and uniform in particle size, good in suspension property, high in polishing speed of precision optical glass, less in scratch, good in wear resistance and remarkable in synergistic polishing effect; therefore, the polishing solution can be applied to the field of high-grade optical instrument processing, and particularly can be used for polishing precision optical glass.
Detailed Description
The present invention will be further described with reference to the following examples. The following description is given by way of example, and the scope of the invention should not be limited thereto.
Example 1:
the specific preparation steps of the implementation are as follows:
A. preparing a colloidal solution:
(1) dispersing 223g of pseudo-boehmite into 2000ml of pure water under the condition of high-speed stirring to obtain solid-liquid mixed slurry;
(2) slowly dripping 75ml of concentrated hydrochloric acid with the mass fraction of 38% into the solid-liquid mixed slurry, and carrying out peptization to obtain an aluminum hydroxide colloidal solution;
(3) dispersing 10.5g of ammonium citrate into an aluminum hydroxide colloidal solution, and uniformly mixing to obtain a colloidal solution A;
B. preparing a mixed system:
(1) dissolving 121g of cerium carbonate by using 38% hydrochloric acid by mass, controlling the pH value of the solution to be 1.3-1.8, and obtaining a cerium chloride solution after complete dissolution;
(2) filtering the cerium chloride solution, and slowly adding the filtered cerium chloride solution into the colloidal solution A to obtain a mixed system B;
C. coprecipitation:
(1) preparing 1mol/L solution of sodium carbonate, and taking 2000ml for later use;
(2) adding a standby 1mol/L sodium carbonate solution into the mixed system B, performing precipitation reaction, controlling the pH value of the solution to be 6.5-7, and after the reaction is finished, performing vacuum filtration and deionized water leaching for three times to obtain a mixed precipitate C;
D. roasting and post-treatment:
(1) placing the mixed precipitate C in a muffle furnace, roasting at 800 ℃, keeping the temperature for 6 hours at constant temperature, and naturally cooling to obtain a polishing powder precursor;
(2) and crushing the polishing powder precursor to ensure that D50 is about 0.8 mu m and D90 is less than 3 mu m, thus obtaining the cerium-aluminum composite oxide polishing powder, wherein the content of cerium is 15 percent and the content of aluminum is 85 percent.
Example 2:
this example is substantially the same as example 1 except that the content of cerium is 10% and the content of aluminum is 90%.
Example 3:
this example is substantially the same as example 1 except that the content of cerium is 50% and the content of aluminum is 50%.
Example 4:
this example is substantially the same as example 1 except that the content of cerium is 30% and the content of aluminum is 70%.
Example 5:
this example is essentially the same as example 1 except that the surfactant is 3.5g cetyltrimethylammonium bromide.
Example 6:
this example is essentially the same as example 1 except that the surfactant is 7g of ammonium oxalate.
Example 7:
this example is essentially the same as example 1 except that the surfactant is 5g of ammonium succinate.
Example 8:
this example is essentially the same as example 1 except that the surfactant is 8.5g ammonium tartrate.
Comparative example 9:
the preparation method adopts the prior art and comprises the following specific steps:
(1) uniformly mixing 233g of pseudo-boehmite, 121g of cerium carbonate and 10.5g of ammonium citrate, placing the mixture in a muffle furnace, roasting at 950 ℃, keeping the mixture at a constant temperature for 6 hours, and naturally cooling to obtain a polishing powder precursor for later use;
(2) and crushing the prepared polishing powder precursor to about 0.8 mu m of D50 by adopting a jet milling mode, wherein D90 is less than 3 mu m, the content of cerium is 15%, and the content of aluminum is 85%.
Table 1 below shows a table of data on the composition, particle size, polishing rate and number of scratches on the surface of a substrate, which was polished to 100cm, of the products obtained in each of the above examples and comparative examples2The silica optical glass of (1).
TABLE 1 comparative data sheet
As can be seen from the data in table 1 above, the polishing effect of example 4 is the best, and the effects of each of the other examples are better than those of comparative example 8, except that the effects of example 2 and comparative example 9 are the same (worst). The cerium and aluminum contents in example 4 with the best effect are 30% and 70%, respectively; the cerium and aluminum contents in example 2, which are the least effective, are 10% and 90%, respectively; polishing effects were 1, 5, 6, 7, 8; although the content ratio of cerium and aluminum in comparative example 8 was the same as that in example 1, the production method thereof was different from that of the present invention, and the effect thereof was the worst. Therefore, the polishing effect of the cerium-aluminum composite oxide polishing powder is related to the content ratio of cerium to aluminum and also related to the production method.
The cerium-aluminum composite oxide polishing powder prepared by the method is suitable for the field of processing of high-grade optical instruments, and particularly can be used for polishing precision optical glass.

Claims (4)

1. A cerium-aluminum composite oxide characterized by being represented by the following general formula xAl2O3-y CeO2Wherein x: y =1 (0.1 ~ 0.5.5), determined by the mass ratio of alumina to ceria in the composite oxide.
2. The preparation method of the cerium-aluminum composite oxide polishing powder is characterized by comprising the following steps:
A. preparing a colloidal solution:
(1) dispersing pseudo-boehmite into a certain amount of pure water under the condition of high-speed stirring to ensure that the mass percentage of the pseudo-boehmite is 10-20 percent, thus obtaining solid-liquid mixed slurry;
(2) slowly dripping concentrated inorganic acid solution into the solid-liquid mixed slurry for peptizing under the condition of keeping the stirring speed unchanged according to the acid/aluminum mass ratio of 0.1-0.45 to obtain aluminum hydroxide colloidal solution;
(3) adding a structure directing agent accounting for 1-3% of the total mass of the powder (pseudo-boehmite and cerium carbonate) into the aluminum hydroxide colloidal solution, and uniformly mixing to obtain a colloidal solution A;
B. preparing a mixed system:
(1) dissolving cerium carbonate in 38 wt% concentrated hydrochloric acid, controlling the pH value of the solution to be 1.3-1.8, and completely dissolving to obtain a clear cerium chloride solution;
(2) filtering the cerium chloride solution, and slowly adding the filtered cerium chloride solution into the colloidal solution A according to the mass percent of aluminum, cerium =1 and (0.1 ~ 0.5.5) to obtain a mixed system B;
C. coprecipitation:
(1) preparing sodium carbonate or ammonium bicarbonate into 1mol/L solution;
(2) adding 1mol/L sodium carbonate or ammonium bicarbonate solution into the mixed system B, performing precipitation reaction, controlling the pH value of the solution to be 6.5-7, and after the reaction is finished, performing vacuum filtration and deionized water leaching for three times to obtain a mixed precipitate C;
D. roasting and post-treatment:
(1) placing the mixed precipitate C in a muffle furnace, roasting at 750-950 ℃, keeping the temperature for 4-8 hours, and naturally cooling to obtain a polishing powder precursor;
(2) and crushing the polishing powder precursor to ensure that D50 is between 0.6 and 1.2 mu m and D90 is less than 3 mu m, thus obtaining the cerium-aluminum composite oxide polishing powder.
3. The method according to claim 2, wherein the concentrated inorganic acid is hydrochloric acid and nitric acid, preferably hydrochloric acid.
4. The method of claim 2, wherein the structure directing agent is an organic ammonium salt such as ammonium oxalate, ammonium succinate, ammonium tartrate, ammonium citrate, cetyltrimethylammonium bromide, and preferably ammonium citrate.
CN201911105224.8A 2019-11-13 2019-11-13 Preparation method of cerium-aluminum composite oxide polishing powder Pending CN110724460A (en)

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CN112126977A (en) * 2020-08-11 2020-12-25 南昌大学 A method for preparing high-purity lamellar single crystal and lamellar dense aggregated cerium carbonate
CN115895453A (en) * 2022-11-10 2023-04-04 湖北五方光电股份有限公司 Polishing solution for infrared cut-off filter and preparation method and application thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112126977A (en) * 2020-08-11 2020-12-25 南昌大学 A method for preparing high-purity lamellar single crystal and lamellar dense aggregated cerium carbonate
CN115895453A (en) * 2022-11-10 2023-04-04 湖北五方光电股份有限公司 Polishing solution for infrared cut-off filter and preparation method and application thereof
CN115895453B (en) * 2022-11-10 2023-09-08 湖北五方光电股份有限公司 Polishing solution for infrared cut-off filter and preparation method and application thereof

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Application publication date: 20200124